Gas chromatography detection method of ethylene glycol, diethylene glycol and menthol in toothpaste

A technology of gas chromatography and detection method, applied in the field of gas chromatography detection of ethylene glycol, diethylene glycol and menthol in toothpaste

Inactive Publication Date: 2013-03-06
HEILONGJIANG PROV LIGHT INDAL SCI RES ACAD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no suitable detection standard for menthol in toothpaste in China

Method used

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  • Gas chromatography detection method of ethylene glycol, diethylene glycol and menthol in toothpaste
  • Gas chromatography detection method of ethylene glycol, diethylene glycol and menthol in toothpaste
  • Gas chromatography detection method of ethylene glycol, diethylene glycol and menthol in toothpaste

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Embodiment Construction

[0031] Below in conjunction with specific implementation example, the present invention will be further elaborated, but do not limit the present invention:

[0032] 1 material

[0033] 1.1 Instrument

[0034] Gas chromatograph: Agilent 6890N

[0035] Autosampler: Agilent 7683B

[0036] Chromatographic column: Agilent DB-624 (30m×0.32mm×1.8μm, 6% cyanopropylbenzene, 94% dimethylsiloxane)

[0037] Detector: Hydrogen Flame Ionization Detector (FID)

[0038] Carrier gas: helium

[0039] 1.2 Reagents and samples

[0040] Methanol: HPLC grade

[0041] Ethylene Glycol: Color Code

[0042] Diethylene glycol: color scale

[0043] L-menthol: standard product ≥98%

[0044] Sample: commercial toothpaste

[0045] 1.3 Standard stock solution

[0046] Accurately weigh 0.25g each of ethylene glycol, diethylene glycol and menthol standard substances, dilute to 50ml with methanol, shake well, prepare standard stock solutions with a concentration of 5mg / ml for each component, and stor...

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Abstract

The invention provides a new technology for simultaneously detecting prohibited substances such as ethylene glycol and diethylene glycol, and functional component menthol in toothpaste by an internal standard method through a gas chromatograph. The method is characterized by comprising the following steps of: adopting an Agilent DB-624 chromatographic column, taking helium as carrier gas, using a flame ionization detector, taking 1,4-butanediol as internal standard substance; and split sampling. Samples are subjected to methanol extraction and ultrasonic oscillation treatment, then stewing, taking a supernatant fluid and filtering by a filtering film with 0.45mu.m, and the filtrate is the sampling solution. Retention time of the sample is used for qualitative analysis, and quantitative analysis is carried out according to a peak area ratio of each component to the internal standard substance. The method has the advantages of high sensitivity, high reproducibility, high selectivity, and strong specificity; the processing method of the samples is simple; through the internal standard method, the analysis error is further reduced; and the method is suitable for qualitatively and quantitatively analyzing ethylene glycol, diethylene glycol and menthol in the toothpaste.

Description

technical field [0001] The present invention is a new technology for simultaneous detection of prohibited substances ethylene glycol and diethylene glycol in toothpaste and menthol, which is a functional component, by using a gas chromatograph, and is suitable for the qualitative determination of ethylene glycol, diethylene glycol and menthol in oral care products such as toothpaste and quantitative analysis. Background technique [0002] Since the domestic toothpaste industry experienced the "diethylene glycol crisis" in 2007, the use of diethylene glycol in toothpaste has been completely banned. And in 2008, the national standard "Standards for Raw Materials for Toothpaste" GB22115-2008 was issued, which clearly stipulates that diethylene glycol and ethylene glycol are prohibited substances. In the finished toothpaste, the sum of diethylene glycol and ethylene glycol brought in by other raw materials as impurities It should be less than or equal to 0.1%; the published nat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 郑伟孙东方李显波孟玉丁海铭
Owner HEILONGJIANG PROV LIGHT INDAL SCI RES ACAD
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